Food Structure 29 (2021) 100202

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Food Structure
journal homepage: www.elsevier.com/locate/foostr

Structural modification on potato tissue and starch using ethanol

pre-treatment and drying process
Jaqueline S. Guedes a, Karoline C. Santos a, Nanci Castanha a, Meliza L. Rojas b,
Manoel D. Matta Junior a, Dâmaris C. Lima a, Pedro E.D. Augusto a, c, *
a
Department of Agri-Food Industry, Food and Nutrition (LAN), “Luiz de Queiroz” College of Agriculture (ESALQ), University of São Paulo (USP), Brazil
b
Dirección de Investigación y Desarrollo, Universidad Privada del Norte (UPN), Trujillo, Peru
c
Food and Nutrition Research Center (NAPAN), University of São Paulo (USP), Brazil

A R T I C L E I N F O A B S T R A C T

Keywords: This work evaluated ethanol as a pre-treatment to the convective drying of potatoes, focused on obtaining their
Drying starch. Potato slices were treated by immersion in ethanol for up to 30 min and then dried by convection (40 ◦ C,
Ethanol 1 m/s). Different treatments were conducted to evaluate the effect of pre-treatment with ethanol and/or drying
Starch
on the potato tissue and starch structure and properties. Potato microstructure, rehydration capacity, and drying
Potato
kinetics were evaluated. After pre-treatment, drying, and rehydration, the starch was extracted and evaluated in
Pasting properties
relation to both structure and properties. Ethanol pre-treatment promoted structural changes on potato tissues
and cells: the cells became withered, with thinner walls, lose turgidity, and changed the initial shape becoming
more distorted and compacted. These permanent structural modifications impacted the subsequent mass transfer:
the drying time was reduced in ~56%, and the initial rehydration rate increased ~25%. There were no changes
in the starch molecular profile and only minor imperfections in the surface of the granules. The starch pasting
and gel properties were only slightly altered by the drying process. In conclusion, drying and its pre-treatment
with ethanol can be a simple technology for preserving potatoes focused on starch extraction.

1. Introduction
Starches are natural biopolymers with great importance as in­
gredients for different industries, such as food, feed, chemical, petro­
chemical, textile, paper and cellulose, adhesives, biodegradable plastics,
among others.
Commercial starches are obtained from sources such as seeds
(mainly maize, wheat, barley, and rice), roots and tubers (mainly cas­
sava and potato). Potato starch is a valued source in different industries,
due to some special properties (Grommers & Krogt, 2009). For instance,
potato starch is used in the food industry due to its high clarity/­
transparency and neutral flavor, and in the textile industry due to its film
properties, adhesive power, and paste penetration depth. In addition,
potato starch is preferred as a pre-coating of filters due to its large
granules, as well as it is also applied in water treatment due to its high
phosphate content. In the paper and cellulose industry, potato starch is
preferred due to its film-forming properties, less moisture retention, and
excellent bonding power (Mitch, 1984).
However, roots and tubers have high moisture content, making them
highly perishable after harvesting, which can result in economic losses if
they are not quickly processed. In fact, although starches from potato
and cassava present interesting industrial applications, they also present
high variability and heterogenicity due to the vegetable senescence and
partial degradation (for example due to fermentation) – which limits
their production and application.
In this context, drying can be a simple, inexpensive, and efficient way
to assure potato preservation focused on starch extraction. Particularly,
convective drying uses hot air to remove the water from the product,
being efficient and simple.
However, this process can take many hours, which is undesirable
from a production perspective, as well as it can negatively impact the
product quality. For instance, the presence of water in starchy raw
materials, the long drying time, combined with the high temperatures,
can promote changes in the starch characteristics, such as its gelatini­
zation properties. Therefore, new approaches are necessary to enhance
potato drying. Moreover, simple approaches are important for

* Corresponding author at: Avenida Pádua Dias, 11, Piracicaba, SP, 13418-900, Brazil.
E-mail address: pedro.ed.augusto@usp.br (P.E.D. Augusto).

https://doi.org/10.1016/j.foostr.2021.100202
Received 3 August 2020; Received in revised form 29 January 2021; Accepted 9 June 2021
Available online 10 June 2021
2213-3291/© 2021 Elsevier Ltd. All rights reserved.
J.S. Guedes et al.
application by small producers.
In fact, ethanol pre-treatment promotes structural modifications and
physical mechanisms that enhance the subsequent drying (Llavata et al.,
2020). In fact, there is growing interest in using the ethanol
pre-treatment to improve drying processes, such as the convective dry­
ing of pumpkin (Carvalho, Massarioli et al., 2020; Carvalho, Rojas et al.,
2020; Rojas, Silveira, & Augusto, 2020), pineapple (Carvalho et al.,
2020; Santos & Silva, 2009; Silva, Braga, & Santos, 2012), bananas
(Corrêa et al., 2012; Silva et al., 2012), carrot (Santos et al., 2021),
melon (Da Cunha et al., 2020), foam mat of pitayas (Araújo et al., 2020)
and guaco (Silva, Celeghini, & Silva, 2018). Moreover, recently the
ethanol pre-treatment started to be studied to improve other drying
techniques, such as the convective drying assisted by ultrasound of apple
(Rojas, Augusto, & Cárcel, 2020), infrared drying of potato (Rojas &
Augusto, 2018b; Rojas, Silveira, & Augusto, 2019) and garlic (Feng
et al., 2019), infrared with hot air in scallion (Wang et al., 2019) and
scallion stalk (Zhou et al., 2020), and vacuum drying of apple (Ama­
nor-Atiemoh et al., 2020).
However, although the high economic and industrial relevance, the
effect of pre-treatment with ethanol and drying on a raw material whose
final product is starch was still not evaluated.
Therefore, the objective of this study was to evaluate the pre-
treatment with ethanol on the convective drying of potatoes, focused
on the subsequent starch extraction. To achieve it, we evaluated the
structural changes in both potato tissues and starch (both granules and
molecules), correlating them with starch properties (pasting and gel),
focusing on structural characteristics and properties of the starch as an
industrial ingredient.
2. Material and methods
This work was divided in different steps. Firstly, potato slices were
obtained and convectively dried, directly or after pre-treatments using
ethanol. In this step, the drying kinetics was evaluated, and the dried
slices were evaluated through their structure and rehydration kinetics.
Next, the potato starch was extracted and purified from the rehydrated
slices. Finally, both structure (granular and molecular) and properties of
the obtained starches were evaluated.
2.1. Sample preparation and ethanol pre-treatments
Potatoes (Solanum tuberosum) were purchased in a local market
(Piracicaba, São Paulo State, Brazil). The tubers were washed and sliced
at 5 mm thick. The fresh potato slices were then submitted to different
treatments before drying: control (D, without any other treatment, being
directly dried just after slicing), ethanol pre-treated for 15 min (E15-D),
and ethanol pre-treated for 30 min (E30-D).
The samples (~300 g) treated with ethanol were immersed in a
beaker containing 1400 mL of ethanol (Êxodo Científica, Brazil) (99.8 %
v/v) for 15 or 30 min, at room temperature (~25 ◦ C). Then, the slices
were removed from ethanol, drained and their surfaces were superfi­
cially dried with absorbent paper. The samples were then weighed and
dried. Pre-treatment times were based on previous works of our research
group (Rojas, Silveira & Augusto, 2020).
2.2. Convective drying
Drying was performed immediately after the pre-treatments, using
air at 40 ◦ C and 1.0 ± 0.1 m s− 1 in a Computer-Controlled Tray Dryer
(Armfield UOP8 Mkll UK). The drying temperature was milder to pre­
vent starch gelatinization.
Potato slices were placed in perforated metal trays, to allow free
circulation of hot air over their surfaces. The potato mass was registered
continuously by a computer connected to the drying tunnel, until con­
stant weight. The drying process was carried out in triplicate.
Drying curves were plotted according to dimensionless moisture
2
Food Structure 29 (2021) 100202
(MR), as described in Eq. (1), where “M” is the moisture content on a dry
basis (% d.b., i.e., kg of water⋅100 kg− 1 dry matter) over the drying time
(t), “Me” is the equilibrium moisture (the average of the last 10 values
obtained after stabilization, % d.b.), and “M0” is the initial moisture (%
d.b.).
Mt − Me
(MRt ) = (1)
M0 − Me
The initial moisture contents (from fresh tubers) and after the pre-
treatment with ethanol were measured by drying crushed potatoes at
115 ◦ C on a moisture analyzer (MX-50, A&D Company, Tokyo Japan).
All moisture data over time were calculated by mass balance, consid­
ering the sample “moisture” is a lumped parameter that includes both
volatile liquids: the remaining water and the absorbed ethanol (Rojas &
Augusto, 2018a). For potatoes without ethanol, the initial moisture was
the same as for fresh potatoes. Therefore, all the curves started with MR
equal to 1.
Page Model was used to evaluate drying, being presented in Eq. (2)
(Page, 1949), where “MR” is the dimensionless moisture, “t” is the
drying time (h), “k” is the drying rate parameter (h− n); and “n” is a shape
parameter (dimensionless). This empirical model has been widely
applied to described food drying. Moreover, Simpson et al., 2017
demonstrated by the anomalous diffusion approach, based on fractional
calculus, some phenomenological interpretation to Page’s parameters:
the parameter “n” is related to the type of diffusion (n = 1 describes
normal diffusion, n ∕ = 1 describes anomalous diffusion with interference
from other phenomena, such as capillarity), while the parameter k can
be associated with the diffusion coefficient and sample geometry.
MR = e− ktn
(2)
2.3. Rehydration process
Rehydration was performed by immersing the dried potato slices in
distilled water at 25 ◦ C ± 1 ◦ C. To avoid water limitation, a ratio of
0.072:1 dry sample:water (w/w) was used. During rehydration, the
samples were removed from the water, drained, and their surfaces were
superficially dried with absorbent paper. They were then weighed and
returned to water until reaching constant weight.
The moisture obtained at each time “Mt” was calculated by mass
balance, considering the initial mass of the sample, the initial moisture
content (M0), and the mass obtained at each time. The rehydration was
performed in triplicate.
Peleg Model (Peleg, 1988) was used to describe the rehydration ki­
netics, being presented in Eq. (3), where “Mt” is the moisture content
over time, “M0” is the initial moisture, “t” is the time, and “k1” and “k2”
are the model parameters. The inverse of k1 describes the rate of water
absorption at the beginning of the process, while the inverse of k2 is
related to the equilibrium moisture content.
t
Mt = M0 + (3)
k1 + k2 ∙t
2.4. Potato structure
Scanning electron microscopy (SEM) was used to observe the struc­
ture of fresh, pre-treated, dried, and rehydrated potato slices. The in­
ternal structure of potato slices was observed, i.e., the surfaces
correspondent to the slice thickness.
For this, rectangular cuts were made in the samples, using a blade
with a smooth comb. After cutting, the obtained pieces were fixed
overnight in 2.5% glutaraldehyde and cacodylate buffer (pH 7.2), to
avoid structural changes during dehydration. Subsequently, the samples
were removed from the solution and washed three times with cacodylate
buffer. Then, the samples were dehydrated in a graded ethanol series
(20%, 40%, 60%, 70%, and 90%) and finally absolute ethanol three
times during 1 h. After the last immersion (using absolute ethanol)
J.S. Guedes et al.
samples were transferred to capsules and washed three times using the
same ethanol. The capsules were placed in a critical point dryer (Leica
EM CPD 300) to remove the solvent without causing changes due to
surface tension in the delicate details of the cells and tissues.
Subsequently, the samples were transferred to stubs, which con­
tained a double-sided carbon tape to hold the samples. The metallization
process deposited a thin layer of gold in the stubs, which were placed in
a scanning electron microscope (LEO 435 VP, Leo Electron Microscopy
Ltd., Cambridge, UK) operating at 20 kV. The samples were then eval­
uated in the microscope using an Earhart-Thornley Detector (ETD) for
secondary electrons and the magnification of 500 × .
2.5. Starch extraction and treatments
The starch extraction was performed according to Castanha, Matta
Júnior and Augusto (2017), with few modifications.
The dried samples (80 g) were rehydrated at 5 ◦ C for 12 h in 1000 mL
of distilled water with the addition of 1 g of potassium sorbate. The
rehydrated slices (200 g) were grounded in a blender with 1 L of water
for 5 min. The obtained suspension was passed through a 250 μm sieve.
The filtrated sample was sieved again using 149, 60, and 50 μm sieves,
and the obtained starch slurry was left to settle for 1 h. The procedure
was repeated 4–5 times until the supernatant became clear. The ob­
tained starch was then oven-dried at 35 ◦ C until reaching ~15 % of
moisture. The obtained starch was then ground in a mortar, sieved
(250 μm), and stored in glass containers until further use.
In order to evaluate the effect of both ethanol pre-treatments and/or
convective drying on starch structure and properties, the evaluated
starch was obtained directly from fresh potatoes (F), and also after pre-
treatments with ethanol for 15 min (E15) and 30 min (E30).
2.6. Starch structure
Both starches granular and molecular structures were evaluated.
Starch granule morphology was evaluated using light microscopy
(Model L10000, Bioval, Curitiba, Brazil; with a 20 W halogen lamp) and
a polarized light filter. The starch was placed on a glass slide, a drop of
Lugol solution (1 % I2 and 2 % KI) was poured, and the system was
covered by a glass slip. The magnification of 400× was used to obtain
the images. Several glass slides were used for the analysis, in order to be
representative.
The starch molecular size distribution was evaluated by gel perme­
ation chromatography (GPC), as described by Song and Jane (2000),
with modifications. A GE XK 26/70 column (2.6 cm diameter and 70 cm
high) packed with Sepharose CL-2B gel (Sigma, Sweden) was used.
Starch samples (0.1 g, on a dry basis) were mixed with 10 mL of
dimethylsulfoxide (DMSO; 90%, Labsynth, Brazil) and gelatinized in
boiling water for 1 h. Then, the solution was kept at 25 ◦ C for 16 h under
constant stirring. Using a pipette, 3 mL of the obtained sample were
blended with 10 mL of absolute ethanol (Êxodo Cientifica, Brazil), and
then centrifuged for 30 min at 3000 g. The supernatant was discarded,
and the precipitated starch was dissolved in 9 mL of boiling distilled
water for 30 min.
In sequence, 4 mL of the gelatinized sample were injected into the
chromatographic column, using a solution of 25 mmol L− 1 of NaCl
(Química Moderna, Brazil) and 1 mmol L− 1 of NaOH (Synth, Brazil) as
mobile phase, at a rate of 60 mL h-1. A fraction collector (Gilson, model
FC203B, Middleton, England) was used to separate the sample into 4 mL
portions. The samples were then evaluated through two techniques: the
blue value (BV) method (Juliano, 1971), and total carbohydrate content
(TCH) by the phenol sulfuric method (Dubois et al., 1956).
In the blue value analysis, 0.12 mL of diluted iodine solution (1.0 g
iodine (Vetec, Brazil) and 0.1 g potassium iodide (Dinâmica Química
Contemporânea, Brazil) in 100 mL of 0.2 M acetate buffer pH 5.0) was
added to 0.025 mL of sample and the absorbance was read using a
spectrophotometer at a wavelength of 620 nm (Femto spectrometer,
3
Food Structure 29 (2021) 100202
Model 600S, São Paulo, Brazil). The analysis of TCH was performed by
adding 25 μL phenol (5% w/v), 125 μL sulfuric acid concentrated
(Cromoline – Química Fina, Brazil) in a 25 μL sample, and the absor­
bance was read at 490 nm.
The blue value method is based on the ability of amylose to form a
helical inclusion complex with iodine, generating a blue color with a
maximum absorption wavelength at 620 nm in the presence of amylose
and purple in the presence of amylopectin (Liu, 2005). The total car­
bohydrate content method determines all carbohydrates in the sample:
the concentrated sulfuric acid disintegrates any large chain carbohy­
drate into monosaccharides. These smaller chain compounds react with
phenol to produce a yellow color (with a maximum absorption wave­
length at 490 nm). In this method, it is possible to analyze changes in the
proportions of amylose and amylopectin that were not complexed with
iodine.
Therefore, changes in molecular size can be described by conducting
both evaluations (blue value and total carbohydrate content) and
comparing the processed starches with the native ones.
2.7. Starch properties
The starches pasting properties were evaluated using Rapid Visco
Analyzer equipment (RVA-4, Newport Scientific Pvt. Ltd., Australia,
with the Thermocline for Windows software, version 3.0). A suspension
of 3 g starch (14% moisture basis) in 25 g of distilled water was analyzed
under constant shear on a programmed heating, retention, and cooling
cycle. The suspensions were initially held at 50 ◦ C for 1 min, heated to
95 ◦ C at 6 ◦ C/min and kept at 95 ◦ C for 5 min, being then cooled to 50 ◦ C
at 6 ◦ C/min, and kept at this temperature for 2 min. The pasting pa­
rameters were then obtained, based on the suspension and paste
apparent viscosity (evaluated in mPa s, where 1 mPa s = 1 cP).
Following, the obtained pastes were stored in plastic cups (40 mm
diameter × 20 mm height) and reserved in a desiccator with water at the
bottom to avoid dehydration. The desiccator was kept at 8 ◦ C for 24 h to
promote gel formation.
The firmness of the obtained starch gels was set by instrumental
texture using a Texture Analyzer (TA. XT Plus, Stable Micro Systems
Ltd., Surrey, UK) with a load cell of 50 kgf (490.3 N). A 0.5” cylindrical
probe (diameter = 1.27 mm) was selected to puncture the sample at
1 mm s− 1 until the penetration depth of 4 mm. The starch gel strength
was determined as the maximum force achieves during the penetration
assay.
2.8. Experimental design, regressions and statistics
A completely randomized design was applied with three process
repetitions. Two analysis repetitions were conducted for each process.
The parameters of Page and Peleg Models were obtained by non-
linear regression using the “Solver” tool from Excel 2016 software
(Microsoft, USA), for each replicate. For this, an error minimization
calculation was made through the quadratic sum of the SSE errors (Eq.
(4)) between the experimental and predicted values. The parameters
were defined as optimal solutions when convergence reached 10− 6.
∑
X
( ( )
SSE = (predicted) − experimental )2i (4)
i=1
Statistic evaluation was conducted using ANOVA and the averages
were compared using the Tukey test using the Minitab software (version
18).
3. Results and discussion
The purpose of this work was not only to study potato drying but also
to understand more deeply the effect of ethanol on drying, rehydration,
and microstructure of vegetables, as well as propose drying of starchy
J.S. Guedes et al.
products as an approach before starch extraction. Consequently, the
obtained results are divided in three sections: (1) effect of ethanol pre-
treatment on potato structure and drying; (2) effect of ethanol on po­
tato rehydration kinetics; and (3) structure and properties of the ob­
tained starches.
3.1. Effect of ethanol pre-treatment on potato structure and drying
The progress of dimensionless moisture content (MR) over the drying
time, for the different treatments, is shown in Fig. 1A.
Pre-treatments with ethanol resulted in faster drying than the control
(D), which can be evaluated by the time needed to achieve a moisture
level of 20 % (on a wet basis). This value represents a moisture level to
achieve microbial stability in dry vegetables (Chen & Patel, 2008). The
necessary time to achieve this level was reduced by ~22% using the
pre-treatment with E15-D min and ~56% for the sample treated with
E30-D min (p < 0.05).
These results are in the same order of magnitudes of previous studies
with other vegetables. Considering convective drying and the pre-
treatment by immersion in ethanol from 10 to 30 min, a reduction in
drying time of 56.9 % was observed in melon (Da Cunha et al., 2020),
51% in carrot (Santos et al., 2021), 34-53% in apples (Rojas, Augusto, &
Cárcel, 2020) and 49-52% in pumpkins (Rojas, Silveira, & Augusto,
2020). At lower intensities of treatment time (such as 5 min of immer­
sion), a reduction in the drying time of pumpkins of 16% was observed
(Carvalho et al., 2020; Carvalho et al., 2020) and 6% in carrot applying
pre-treatment for 3 min.
Regarding the application of ethanol on the sample surface, a
Fig. 1. (A) Convective drying (40 ◦ C, 1.0 m/s) of potato slices with different treatments: control and drying after pre-treatments with ethanol for 15 and 30 min.
Results represent the mean ± standard deviation of treatments of the experimental data. The inserted graphic shows the time required for all treatments to reach the
final moisture of 20 % w.b. (average ± standard deviation). Down arrows represent the percentage time reduction among treatments. (B) Page Model parameters (Eq.
(2)). Results represent the mean ± standard deviation of treatments.
4
Food Structure 29 (2021) 100202
reduction of 6–34% was observed in banana, pineapple, and apple,
while this reduction was from 7 to 17% when ethanol was applied in the
drying atmosphere (Santos & Silva, 2009; Silva et al., 2012).
Different possibilities can explain the effect of ethanol in reducing
drying time.
Firstly, ethanol can promote structural changes (Corrêa et al., 2012;
Rojas & Augusto, 2018a, 2018b; Wang et al., 2019). When in contact
with food, ethanol causes the extraction of water and other components,
as well as the incorporation of ethanol, resulting in structural changes.
These effects can be evidenced by Fig. 2, which shows SEM images of
potato slices after pre-treatment, after drying, and after rehydration. In
these images, it is possible to observe that after the pre-treatments with
ethanol, the cells became withered in comparison with the control. After
rehydration, the thinner cells can be better noticed. In fact, ethanol
extracts some components of cell walls and/or membrane, which
became thinner. Moreover, the cells lose turgidity, changing its initial
shape, and becoming more distorted and compacted. These permanent
structural modifications can facilitate the entry of water during hydra­
tion, even though ethanol is not in the sample anymore. Similarly, this
indicates water can leave the product easily during drying. More in­
formation about those processes is described as follows.
The vegetable cell wall and membrane have a diversified composi­
tion. According to Canteri et al., 2019, ethanolic solutions can extract
polyphenols, some classes of proteins, and lipids from cell walls and/or
membranes. On the other hand, the compounds related to the cell wall
structure, such as cellulose, lignin, or hemicellulose, are not extracted.
Therefore, once the overall cell structure is maintained, but with thinner
walls, it avoids collapsing and ensures enhanced water flux through it
J.S. Guedes et al. Food Structure 29 (2021) 100202

Fig. 2. Structural changes inside the potato slices before drying, after drying and rehydration of each treatment. Images obtained by scanning electron microscopy
(SEM) with magnifications of 500× (the inserted yellow bars represent 100 μm).

Fig. 3. Representative scheme of pre-treatment with ethanol prior to drying of vegetables.

5
J.S. Guedes et al.
during both drying and rehydration processes.
Moreover, once starch granules are not soluble in ethanol, they are
not extracted during pre-treatment – which is important if the objective
is to obtain starch. However, ethanol can modify starch – the reason why
we added three more treatments in the evaluation: (F), (E15), and (E30),
which were starches extracted from potatoes before and after pre-
treatments with ethanol, without drying.
Therefore, structural modifications caused by ethanol can affect both
vegetable drying and rehydration. In fact, the effect of ethanol on food
product structure is still beginning to be described, but the changes
caused by it in the drying process are remarkable, as discussed as
follows.
Another possible mechanism to explain the effect of ethanol pro­
moting structural changes is the osmotic dehydration caused by it. Os­
motic dehydration is based on the removal of water by direct contact of
the food material with a hypertonic medium. In this case, the cell wall
acts as semipermeable membranes that allow the passage of small
molecules, such as water (Shi & Le Maguer, 2002). Therefore, the dif­
ference in osmotic pressure between ethanol and the vegetable (intra­
cellular and intercellular content) can remove part of the product’s
water. In fact, according to Wang et al. (2019), pre-treatments using
ethanol and vacuum promoted osmotic dehydration of scallion.
A third explanation for ethanol improving drying is due to its
interaction with the water in the food. Ethanol increases the sample
vapor pressure and promotes the Marangoni effect.
The Marangoni Effect was first described by Thomson (1855), being
associated with food drying by Silva et al. (2012). It constitutes a mass
flow mechanism associated with the difference in the surface tension. In
the present work, the Marangoni Effect occurs both during
pre-treatment and drying (Fig. 3). During the pre-treatment, ethanol
enters the potato slices and water flows from the food to ethanol. The
food surface is then composed of a mixture of water and ethanol. Due to
the lower boiling point of ethanol, it evaporates faster than water during
drying, leaving more water than ethanol on the surface. As ethanol
concentration is reduced in the sample surface during drying, this region
reaches a higher surface tension in relation to the layers below. This
gradient in surface tension pulls the fluid from the next layer. It results in
a continuous flow within the adjacent inner layers of the food to the
surface, which happens until a balance of surface tension is achieved
(Rojas & Augusto, 2018a).
In the present study, the combination of structural changes, osmotic
dehydration, and the Marangoni Effect can explain the success of etha­
nolic pre-treatment in reducing potato drying time.
Page Model was empirically proposed by MSc. Glen Page in 1949
(Page, 1949) in order to improve the fitting of experimental drying data.
After that, a phenomenological explanation was proposed by Simpson
et al. (2017). According to the authors, the parameter “k” is associated
with the effective diffusivity and sample geometry, while the parameter
“n” is related to the microstructure of the food and the mechanism of
mass transfer (the type of diffusion). When n>1, the process is charac­
terized as super-diffusive, while when n<1, the process is sub-diffusive.
Analyzing the parameters of the Page Model (Fig. 1B), an increase in
the “k” parameter is noticeable for the E30-D treatment, whose value
was 108% higher than the “D” treatment. By representing an increase in
the drying rate, this is consistent with the mass transfer improvement.
The parameter “n” had values always greater than 1, demonstrating a
super-diffusive behavior (n>1). This is similar to the convective drying
of pumpkin (Rojas, Silveira, & Augusto, 2020) and apple (Rojas,
Augusto, & Cárcel, 2020), and infrared drying of potato (Rojas &
Augusto, 2018b). This indicates the presence of other phenomena
involved during mass transfer in relation to pure diffusion, such as
capillarity and the Marangoni Effect. Although “n” values did not show
differences among treatments by considering p = 0.05, it so with
p = 0.2. This indicates although ethanol accelerates drying, the overall
super-diffusive behavior is not affected.
Therefore, ethanol reduced the drying time, which is interesting and
6
Food Structure 29 (2021) 100202
desirable. However, ethanol can affect starch structure and properties,
which can impair product quality. Consequently, its evaluation becomes
necessary, as discussed in the following sections.
3.2. Effect of ethanol on potato rehydration kinetics
Fig. 4 shows the rehydration kinetics of potato slices after different
pre-treatments and convective drying, as well as the associated Peleg
Model (Eq. (3)) parameters, “k1” and “k2”.
Ethanol treatments showed slightly faster rehydration at the begin­
ning of processing, whose behavior becomes similar to the control as the
processing time is increased. Therefore, smaller values (p < 0.05) for
“k1” were achieved using the pre-treatments with ethanol (Fig. 4). This
result is interesting since rehydration would be the first step in starch
extraction. Moreover, this effect can be associated with the structural
changes caused by ethanol (Section 3.1), which facilitates the water flow
into the sample due to modifications in the cell wall.
This result is in line with those reported for convective drying of
pumpkins (Rojas & Augusto, 2018a; Rojas, Silveira, & Augusto, 2020),
or even other drying strategies, such as infrared and vacuum drying of
scallion (Wang et al., 2019), microwave-assisted drying of apple slices
(Funebo et al., 2002) or ultrasound-assisted convectively dried (Rojas,
Augusto, & Cárcel, 2020). All these works described the positive impact
of ethanol on the rehydration properties.
However, a different behavior to this rehydration kinetics was
observed when potato slices were dried using infrared radiation by Rojas
and Augusto (2018b) and Rojas et al. (2019). In the mentioned works,
the ethanol pre-treatment negatively affected the potato rehydration.
However, that studies were conducted using infrared drying, whose
mechanisms of heat transfer and the temperature reached by samples
are different. In that works, samples reached higher temperatures,
causing the formation of crust, and hindering the potato rehydration
process. Therefore, in those cases, ethanol can negatively impact this
crust formation during infrared drying, then decreasing the drying rate.
On the other hand, those problems were not evidenced in the present
work, using convective drying. Moreover, convective drying is a method
much simpler and cheap than infrared drying. In fact, convective drying
can be performed even by small farmers, which can achieve potato
preservation at low costs and through a simple approach – even
considering the pre-treatments with ethanol. Therefore, we highlight
once again this is an interesting result, given obtaining starch as a final
product.
For the parameter “k2”, no differences were evidenced among
treatments (p > 0.05). As observed in the hydration curve (Fig. 4), all
treatments had the same profile and achieve similar moisture contents at
the end of rehydration. Even so, the achieved equilibrium moisture was
always ~70% of the original moisture (i.e., the in natura potatoes):
~72% (2.64 kg water/ kg dry matter) for the D treatment, ~71%
(2.47 kg water/ kg dry matter) for the E15-D and 72% (2.63 kg water/
kg dry matter) for E30-D.
A possible explanation for this behavior is associated with changes in
structure and air presence. After drying, some air can get trapped inside
the pores, forming bubbles that can obstruct the water flow (Saguy,
Marabi, & Wallach, 2005). This is very common in dry products, where
the structural changes reduce the ability to accommodate water in
relation to the fresh product (de Moraes, 2018).
Once again, the rehydration results of this work are better than those
obtained by the infrared drying of potatoes pre-treated with ethanol
(Rojas & Augusto, 2018b; Rojas et al., 2019): in these two works,
ethanol pre-treatment reduced the equilibrium moistures after rehy­
dration, when compared with the control drying. Once again, the effect
of convective drying on potatoes in relation to infrared drying stands
out.
However, the results here obtained for potatoes are different from
those obtained for other vegetables, highlighting the differences among
vegetable matrixes. The pre-treatment with ethanol (Rojas & Augusto,
J.S. Guedes et al. Food Structure 29 (2021) 100202

Fig. 4. Up: Rehydration kinetics (25 ◦ C) of potato slices after pre-treatments (D, E15-D, and E30-D) and convective drying (40 ◦ C). Dots are experimental data and
bars are ± standard deviation over rehydration time. The dotted line represents the in natura potato moisture. The Peleg Model (Eq. (3)) is represented by the dotted
curves. Down: Parameters of Peleg Model for the rehydration kinetics. Results represent the mean ± standard deviation of treatments.

2018a) resulted not only in a higher rehydration rate in pumpkins but
also higher equilibrium moisture content – which was closer to the in
natura moisture when compared with the control. Moreover, some
studies showed equilibrium moisture contents higher than the fresh
product. For example, Rojas, Augusto, & Cárcel (2020) described
rehydrated apples presented moisture ~5% higher than the fresh
product when ethanol pre-treatment was applied. For comparison, the
control treatment obtained a final moisture ~6% lower than the fresh
product. Once more, these differences can be associated with differences
in composition and structure among the products, where their tissues
and the ways in which they are arranged can influence the drying and
rehydration properties.
In summary, the results presented in this section are interesting as
they reveal that ethanol treatment did not negatively affect the
rehydration properties. On the contrary, the longer contact time with
ethanol provided a higher rate of rehydration. Furthermore, it does not
indicate crust formation due to starch gelatinization. However, the
structure and properties of the resulted starches must be evaluated, as
described in the next sections.
3.3. Structure and properties of the obtained starches
Starch was extracted and evaluated before pre-treatment, after pre-
treatment, and after rehydration of dry potato slices. The granular and
molecular structure of starches are factors that will determine their
functional properties. Therefore, we first analyzed the effect of pre-
treatments and drying on the starch structure and then on their prop­
erties. Accordingly, this section organizes these results into two sub-

Fig. 5. Molecular size distribution profiles of potato starch after different treatments: The first three samples correspond to the starch extracted from potatoes
without drying (F, E15, E30) and the last three correspond to starch extracted from dried potatoes (D, E15-D, E30-D). After gel permeation chromatography (GPC),
the molecular profiles were based on the samples’ total carbohydrates (A) and blue value (B) techniques.

7
J.S. Guedes et al. Food Structure 29 (2021) 100202

sections: starch structure (molecular and granular structure), and starch

properties (paste and gel properties).

3.3.1. Starch structure: molecular and granular structure

The results of gel permeation chromatography (GPC) for starches
extracted from dried potatoes and after pre-treatments (before drying)
are shown in Fig. 5 (for both the blue value (BV) and total carbohydrates
(TCH) methods).
The blue value (BV) analysis is based on the ability of starch to form a
helical inclusion complex with iodine. Consequently, this iodometric
method only covers long and medium chains of α (1→4) – glucan con­
tents, mainly amyloses (Liu, 2005). The phenol-sulfuric method can
measure all the carbohydrate content (TCH) present in the sample.
Combining both methods is an interesting approach to evaluated
modified starches.
Both the results of TCH and BV (Fig. 5) present a first large peak
(corresponding to amylopectin) and a second small and wide peak
(amylose), for all treatments. Moreover, the curve profile and order of
magnitudes are the same for all treatments. This indicates the size of the
potato starch molecules was not affected by any process here described
(ethanol pre-treatment and/or convective drying).
It is worth mentioning this is an excellent result from a starch
extraction point of view, as it shows the molecular fractions were not
affected by processing. This indicates that drying can be used for potato
preservation with the objective of subsequent starch extraction – at least
in the conditions here evaluated. However, starch properties must also
be evaluated once the rheological properties are greatly influenced by
factors such as amylose/amylopectin ratio and the length of their chains.
Changes in these factors would imply a change in the characteristics of
the paste and the gel formed (Liu, 2005).
Starches are organized in structures called granules, which are
different in size and shape. Starch granules from tubers are mostly bulky
and oval-shaped with an eccentric hilum, and potato starch has the
largest granules of all starches (Liu, 2005). Light microscopy was per­
formed, with and without a polarized filter, to evaluate starch granule
structures. The results are presented in Fig. 6.
No changes were observed between starches extracted from potatoes
after pre-treatment (E15 and E30) and from fresh potatoes (F). There­
fore, apparently, the application of ethanol to the potato slices did not
alter the starch granules. This result is different from those reported by
Sarifudin et al., (2020), who observed that potato starches had their Fig. 6. Microscopic images of the potato starch granules extracted before and
structure drastically altered when immersed in ethanol in the temper­ after drying without and with polarized filter (left and right column, respec­
tively), and with different pre-treatments: starches extracted from potatoes
ature ranges of 90 ◦ C–100 ◦ C. However, their work was conducted by
before drying (F, E15, E30), and starches extracted from dried potatoes (D, E15-
immersing the isolated starch into hot ethanol, which is a condition
D, E30-D). Images from light microscopy, where the red line represents 40 μm.
much more drastic than in the present work. In the present work, the The red arrows indicate granule imperfections.
potato slices were immersed in ethanol at room temperature, while the
starch granules were still protected inside the cells.
gelatinization (Thomas & Atwell, 1999); therefore, no evidence of
In addition, the mild drying conditions (40 ◦ C), can also explain the
gelatinization was observed in the present study. Even so, the starch
small changes in granule structure (Fig. 6D, E15-D, and E30-D). Even so,
properties must be assessed in order to evaluate possible applications
some imperfections, as small “scratches”, are observed in the granules of
and also possible limitations of the present approach.
starches extracted from dried potatoes. These scratches could indicate
Few studies evaluated starch structure and properties after vegetable
the granules started to shrink and crack due to water loss during drying.
drying. Recently, Duan et al., (2020) conducted different types of drying
In fact, according to (Liu, 2005), starches with crystalline pattern type B,
of Yam: convective drying and microwave freeze drying, also using the
such as potato, have a significant amount of water in their crystalline
ultrasound pre-treatment. The authors reported the convective drying at
regions, and these granules are expected to shrink and crack during
milder temperatures (40 ◦ C, and 50 ◦ C) did not alter the molecular
dehydration. Probably what prevented the granules from collapsing was
distribution of starch. However, according to the authors, drying at
the fact they were protected inside the potato tissues and the relatively
higher temperatures (60 ◦ C, 70 ◦ C, and 80 ◦ C) resulted in molecular
low temperature used for drying.
degradation. However, the authors did not analyze the granular struc­
Using polarized light under a microscope, a typical birefringence
ture of yam’s starch, which could indicate changes due to the gelatini­
cross is seen as two intersecting parts, called Maltese Crosses. This in­
zation process, for example.
dicates there is a radial orientation of the crystallites or there is a high
Therefore, no changes were observed in the structure of the starch
degree of the molecular order within the granules (Liu, 2005). As shown
granules and molecules. However, starch properties must also be
in Fig. 6 (with polarized filter), there were no changes in the granules’
evaluated.
Maltese Crosses: all treatments showed the characteristic behavior of
potato starch. This can indicate the observed imperfections are only
superficial. Moreover, the loss of birefringence is an indicator of

8
J.S. Guedes et al.
3.3.2. Starch properties: pasting and gel properties
The starches’ pasting properties are an important evaluation not only
to characterize starch samples but also to illustrate possible changes in
modified starches when compared to their native form. The pasting
profiles are shown in Fig. 7A, and their main parameters are presented in
Table 1.
The RVA consists of a heating, holding, and cooling procedure,
where the starch suspension is gelatinized forming the paste. During the
heating period, the granule absorbs water, and the suspension apparent
viscosity starts to increase. The temperature when the apparent viscosity
starts to increase is called pasting temperature (PT). When enough
granules are swollen, a rapid increase in apparent viscosity occurs, being
the maximum value called the peak apparent viscosity (PAV). At this
point, there is an equilibrium between the swelling of granules and the
leaching of polymers (Balet et al., 2019).
As the temperature rises further and remains constant, the swollen,
hydrated granules begin to rupture, leaching amylose and small
amylopectin molecules. It is followed by an alignment of the polymers,
decreasing the paste apparent viscosity until the called Trough Apparent
Viscosity (TAV). This step is known as Breakdown (BD), and this
parameter represents the difference between PAV and TAV.
Subsequently, cooling occurs, promoting the re-association of starch
molecules, mainly amylose, and increasing consistency until the final
apparent viscosity (FAV). This process is called Setback (SB) and in­
volves the molecular re-association of starch molecules (Balet et al.,
2019).
All those six parameters are shown in Table 1. The results concerning
the fresh (F) and control (D) samples are similar to those reported for
potato starch in the literature (Castanha, Matta Junior, & Augusto,
2017; Liu et al., 2007; Noda et al., 2005).
The starches extracted after the pre-treatments with ethanol (E15
and E30) showed slightly lower PT than the other treatments. There was
no difference among all treatments regarding PAV values. These results
reinforce the hypothesis that the observed abnormalities in the granules
after drying (Fig. 6) were not so deep as to break the granules, since if
there were deep cracks, it would affect the granule’s resistance, affecting
the PAV.
After the granules rupture, the leached polymers alignment is
described by the parameter Breakdown (BD - being calculated through
the difference between PAV and TAV). As the BD represents the absolute
difference between PAV and TAV, and as both parameters change, it is
more appropriate to evaluate the Relative Breakdown - calculated from
the BD difference and the PAV values (Castanha, Matta Junior, &
Augusto, 2017). In this work, the starches obtained from dried potatoes
have lower RBD and higher FAV values, due to higher TAV values
(p < 0.05).
The results indicate the paste obtained from dried potatoes is slightly
Fig. 7. (A) Potato starch pasting profile: RVA curves obtained from starches extracted from potatoes before drying (F, E15, E30), and starches extracted from dried
potatoes (D, E15-D, E30-D). (B) Gel firmness from the starches extracted from potatoes before drying (F, E15, E30), and starches extracted from dried potatoes (D,
E15-D, E30-D). Variations followed by the same letters do not differ significantly (p > 0.05).
9
Food Structure 29 (2021) 100202
more consistent than those obtained from potatoes without drying (in
special due to the FAV parameter). Low FAV and RSB could indicate a
low rate of starch retrogradation (Shafie et al., 2017). Although no
major differences were observed on starch granules nor molecules, this
suggests the molecules had a different tendency to align. This could also
indicate stronger gels. However, the gel properties must also be evalu­
ated, as discussed as follows, once the results obtained from RVA only
describe a partial alignment (it is important to remember that FAV is
measured at 50 ◦ C).
These results differ from those described by Duan et al. (2020), in
which the pasting properties of starches obtained from dried yams differ
widely from fresh vegetables. Despite being a starch different from po­
tato starch, an important step in Duan et al. (2020) work can influence
their results: before drying, their samples were blanched in a boiling
water bath, which can affect starch and their pasting properties.
Therefore, a direct comparison cannot be carried out.
After obtaining the paste in the RVA, a gel structure is formed during
storage at reduced temperature. The firmness of the obtained potato
starch gels is shown in Fig. 7B. No differences (p = 0.05) were observed
among the starches obtained from dried potatoes (D, E15-D, and E30-D)
and the starch obtained from fresh ones (F), – possibly due to the high
standard deviations. Even so, a tendency of slightly stronger gels from
dried potatoes is observed – for instance, the treatment E30-D is stronger
than the F potatoes at p = 0.10.
Once any important difference was observed in starch molecules
(Fig. 6), the observed trend (slightly stronger gels and pastes from
starches obtained from dried potatoes) can be possibly associated with
the remained ghosts.
The starch ghosts are defined as gelatinized starch granule envelopes
after the majority of internal starch polymers have been released, being
associated with the traces of protein bounded in granules and influ­
encing pasting and gel properties (Han & Hamaker, 2002). Therefore,
probably it is not only a coincidence a correlation between the super­
ficial imperfection in dried granules (Fig. 6) and the trend for stronger
gels (Fig. 7B).
Similarly, there were also no differences between starches obtained
after pre-treatment (E15 and E30) in relation to fresh potatoes (F,
p < 0.1), although a tendency of weaker gels is suggested for the starches
obtained after ethanol pre-treatment in relation to those obtained from
dried potatoes.
Even though, the obtained result is interesting since both behaviors
would be interesting from an industrial perspective: obtaining starches
with any difference from the control or obtaining stronger gels. This
makes drying an option for preserving potatoes whose starch would be
used with application in gels.
In summary, drying showed some effects on starch granule surface
and in some pasting properties parameters. However, these effects were
J.S. Guedes et al.
Table 1
Pasting properties of starches extracted from potatoes before drying (F, E15, E30), and starches extracted from dried potatoes (D, E15-D, E30-D).
Treatments PAV (mPa s)
a b
Starches obtained from fresh potatoes F 10052 ± 160.0
E15 10437 ± 157.8a
Starches obtained from potatoes after pre-treatments
E30 11407.5 ± 9.2a
D 10309 ± 299.0a
Starches obtained after drying E15-D 10240 ± 425.0a
E30-D 11039 ± 875.0a
Average ± standard deviations. The same small letters within a column do not differ significantly (p > 0.05). Peak Apparent Viscosity (PAV), Trough Apparent
Viscosity (TAV), Relative Breakdown (RBD), Final Apparent Viscosity (FAV), Relative Setback (RSB) and Pasting Temperature (PT).
low and did not change the overall starch properties profile. Conse­
quently, the proposed treatments can be used to prolonging the stability
of potatoes tubers, without significantly impacting their starch
properties.
4. Conclusions
The use of pre-treatment with ethanol promoted structural changes
in potato tissues and cells, improving the subsequent water flow during
drying and rehydration. This pre-treatment reduced the drying time up
to ~56% and increased the initial rehydration rate up to ~25%. Possible
mechanisms were discussed, including the structural changes and
physical mechanisms.
No changes were observed on the starch molecular profile, and low
imperfections were observed in the granule surface of starches extracted
from dried potatoes. Slight changes were observed in the properties of
starches extracted from dried potatoes and after the pre-treatment.
Therefore, we can conclude the ethanol pre-treatment and convec­
tive drying can be an interesting option to increase the potato tubers
shelf life for later starch extraction.
CRediT authorship contribution statement
Jaqueline S. Guedes: Conceptualization, Methodology, Validation,
Formal analysis, Investigation, Data curation, Writing - original draft,
Visualization. Karoline C. Santos: Methodology, Formal analysis,
Investigation, Data curation. Nanci Castanha: Methodology, Formal
analysis, Data curation, Writing - review & editing, Visualization.
Meliza L. Rojas: Methodology, Formal analysis, Data curation, Writing -
review & editing, Visualization. Manoel D. Matta Junior: Methodol­
ogy, Formal analysis, Investigation. Dâmaris C. Lima: Methodology,
Formal analysis, Investigation, Data curation. Pedro E.D. Augusto:
Conceptualization, Methodology, Formal analysis, Resources, Writing -
review & editing, Supervision, Project administration, Funding
acquisition.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
The authors are grateful to the São Paulo Research Foundation
(FAPESP, Brazil) for funding the project nº 2019/05043-6; this study
was financed in part by the “Coordenação de Aperfeiçoamento de Pes­
soal de Nível Superior - Brazil (CAPES)” – for the JS Guedes
(88882.378356/2019-01) and KC Santos (88882.378385/2019-01) M.
Sc. scholarships; to the National Council for Scientific and Technological
Development (CNPq, Brazil) for the JS Guedes M.Sc. scholarship
(131235/2020-6) and the productivity grant of PED Augusto (306557/
2017-7); and to the Fondo Nacional de Desarrollo Científico, Tec­
nológico y de Innovación Tecnológica (FONDECYT, Peru) from the
10
Food Structure 29 (2021) 100202
TAV (mPa s) RBD (%) FAV (mPa s) RSB (%) PT (◦ C)
a b a
2793.5 ± 20.5 72.0 ± 0.6 3637.5 ± 70.0 30.2 ± 1.6 66.9 ± 0.8ab
2378 ± 148.9b 77.2 ± 1.1a 3290 ± 48.8b 38.6 ± 7.1a 63.8 ± 0.3c
2643 ± 70.7b 76.8 ± 0.6a 3560 ± 7.1b 34.7 ± 3.9a 64.4 ± 0.0bc
3557 ± 306.0a 65.5 ± 2.6b 4688 ± 331.0a 31.9 ± 2.8a 68.9 ± 1.6a
3812.6 ± 153.4a 62.7 ± 2.9b 5014 ± 220.4a 32.4 ± 4.0a 68.6 ± 0.3a
3770 ± 247.0a 65.8 ± 1.6b 4982 ± 257.0a 32.3 ± 3.3a 68.2 ± 0.4a
“Consejo Nacional de Ciencia, Tecnología e Innovación Tecnológica”
(CONCYTEC, Peru) for funding the project n◦ 409-2019-FONDECYT.
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